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Preparation method of polyimide multilayer composite film containing inorganic nanopowder

A multi-layer composite film and inorganic nanotechnology, which is applied in the field of insulating materials and heat resistance, can solve the problems of reduced mechanical properties, achieve convenient operation, avoid stress concentration, and improve mechanical properties

Inactive Publication Date: 2011-12-07
HARBIN UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method solves the problem that the mechanical properties of the polyimide film are reduced after the introduction of inorganic fillers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) 5g of nano-silica, 0.5g of 3-aminopropyltrimethoxysilane and 60ml of absolute ethanol were stirred at 60°C and carried out intermittent ultrasonication after drying, and the reflux reaction was completed after 0.5 hours. The reacted nano-powder is washed with absolute ethanol, then dried in an ordinary oven for 5 hours, taken out, ground with a mortar and put into a desiccator for standby.

[0023] (2) Dissolve 2.84g of 4,4'-diaminodiphenyl ether in 50ml of N,N-dimethylacetamide, stir at a certain speed to dissolve completely, and then add 3.12 g pyromellitic dianhydride to prepare a polyamic acid solution with high molecular weight.

[0024] (3) Dissolve 0.15 g of the nano-silica powder prepared in step 1 in 10 ml of N, N-dimethylacetamide, and add it to the polyamic acid solution dropwise after ultrasonic dispersion for 30 minutes, and continue Stir mechanically for 1 hour.

[0025] (4) After filtering the glue, first place the polyamic acid glue containing inor...

Embodiment 2

[0030] (1) Stir 5g of dried nano-titanium dioxide, 0.25g of 3-methacryloxypropyltrimethoxysilane and 40ml of absolute ethanol at 70°C and perform intermittent ultrasonication, and condense and reflux for 2 hours At the end, the reacted nano-powder is washed with absolute ethanol, then dried in an ordinary oven for 5 hours, taken out, ground with a mortar and put into a desiccator for later use.

[0031] (2) Dissolve 2.74g of 4,4'-diaminodiphenyl ether in 40ml of N,N-dimethylacetamide, stir at a certain speed to dissolve it completely, and then add 3.06 g pyromellitic dianhydride to prepare a polyamic acid solution with high molecular weight.

[0032] (3) Dissolve 0.10 g of nano-titanium dioxide prepared in step 1 in 20 ml of 4,4′-diaminodiphenyl ether, use ultrasonic dispersion for 1 hour, and then add it dropwise to the polyamic acid solution, and continue mechanical stirring for 1 hour Hour.

[0033] Carry out film laying by the method described in step (4) (5) (6) (7) in ...

Embodiment 3

[0035] (1) Stir the dried 5g of nano-alumina, 0.2g of vinyltriethoxysilane and 50ml of absolute ethanol at 80°C and perform intermittent ultrasonication, condensing and refluxing the reaction for 4 hours to end, and the reacted The nanopowder is washed with absolute ethanol, then dried in an ordinary oven for 5 hours, taken out, ground with a mortar and put into a desiccator for later use.

[0036] (2) Dissolve 2.6g of 4,4'-diaminodiphenyl ether in 40ml of N,N-dimethylacetamide, stir at a certain speed to dissolve it completely, and then add 2.96g Pyromellitic dianhydride to prepare a polyamic acid solution with high molecular weight.

[0037] (3) Dissolve 0.2 g of the nano-alumina prepared in step 1 in 30 ml of N, N-dimethylacetamide, and use ultrasonic dispersion for 20 minutes to add dropwise to the polyamic acid solution, and continue mechanical stirring for 1 Hour.

[0038] According to the method described in step (4)(5)(6)(7) in Example 1, film laying, the thermal imi...

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Abstract

The invention discloses a preparation method of a polyimide multilayer composite film containing inorganic nanometer powder. Polyimide composites containing inorganic nano-powders often reduce the mechanical properties of the film, especially when the nano-powders are not uniformly dispersed, the reduction in film performance is more significant. The present invention includes: (1) pretreatment of inorganic nanopowder; (2) taking 4,4'-diaminodiphenyl ether and pyromellitic dianhydride as raw material monomers and dissolving them in a solvent to polymerize and generate polyamic acid solution; (3) ultrasonically disperse the pretreated inorganic nano-powder in a solvent, and add it to the polyamic acid solution to prepare a polyamic acid solution containing the inorganic nano-powder; (4) prepare the polyamic acid solution containing the inorganic nano-powder The solid polyamic acid solution and the pure polyamic acid solution are filmed in sequence; (5) the film is placed in an oven at 50-400°C for thermal imidization treatment to obtain polyimide containing inorganic nano-powder Hybrid multilayer composite film. The invention is used for preparing polyimide multilayer composite film containing inorganic nanometer powder.

Description

Technical field: [0001] The invention relates to a heat-resistant and insulating material, in particular to a preparation method of a polyimide multilayer composite film containing inorganic nanometer powder. Background technique: [0002] Polyimide is a ring-chain polymer compound containing an imide ring structure in the main chain of the molecule, and is a heterocyclic compound with a semi-ladder structure. Due to the aromatic ring in the framework, the polymer has higher thermal stability, and it is also the polymer material with the highest heat resistance level in industrial applications so far. Because there are very stable aromatic heterocyclic structural units in the polyimide molecule, it has excellent thermal properties, mechanical properties and electrical properties unmatched by other polymers, so it is widely used in electrical insulation, aerospace and microelectronics industries. and other fields have been widely applied. However, with the development of sc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08
Inventor 刘立柱武天祥翁凌周佩君朱兴松高琳宋玉侠杨立倩
Owner HARBIN UNIV OF SCI & TECH
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